CN105230626A - Aminopyralid and clopyralid compounding aqueous agent and preparation method thereof - Google Patents
Aminopyralid and clopyralid compounding aqueous agent and preparation method thereof Download PDFInfo
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- CN105230626A CN105230626A CN201510623912.9A CN201510623912A CN105230626A CN 105230626 A CN105230626 A CN 105230626A CN 201510623912 A CN201510623912 A CN 201510623912A CN 105230626 A CN105230626 A CN 105230626A
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- clopyralid
- aminopyralid
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Abstract
The invention provides an aminopyralid and clopyralid compounding aqueous agent and a preparation method thereof, and relates to the technical field of prevention and control of annual broadleaf weeds in brassica campestris fields, wherein the aminopyralid and clopyralid compounding aqueous agent is prepared from 6 parts by weight of aminopyralid, 24 parts by weight of clopyralid, 3 parts by weight of fatty alcohol polyoxyethylene ether, 5 parts by weight of styryl phenol polyoxyethylene ether, and 62 parts by weight of deionized water. The preparation method comprises: pumping all raw materials into a preparing kettle, carrying out mixing stirring, carrying out primary grinding through a colloid mill, carrying out fine grinding through a sand mill, sampling and analyzing, filtering after qualifying, metering, packaging, and warehousing. According to the present invention, the aminopyralid and clopyralid compounding aqueous agent provides excellent prevention and control effects on annual broadleaf weeds in brassica campestris fields, the significant synergetic effect of the aminopyralid and the clopyralid can be achieved, the suspension rate, the persistent foaming property, the wet sieve test, the thermal storage stability and other performances of the aminopyralid and clopyralid compounding aqueous agent are significantly superior to the performances of the products prepared according to other ratios, and the significant synergetic effect can be provided when the compounded 30% aminopyralid and clopyralid compounding aqueous agent according to a ratio of 1:4 is subjected to mixing use.
Description
Technical field
The present invention relates to the annual broadleaf weed Prevention Technique field of Rapeseed Field, specifically relate to a kind of picloram and clopyralid compound aqueous and preparation method thereof.
Background technology
At present, the weed killer herbicide of the existing annual broadleaf weed for preventing and treating Rapeseed Field, such as " CN104381296A " discloses one " Herbicidal combinations containing picloram and glyphosate ", adopts weight ratio to be that the picloram of 1:5 ~ 5:1 and glyphosate carry out composite Chinese patent.Separately there is Chinese patent " CN102326557A " to disclose one " Herbicidal combinations containing azoles humulone and clopyralid ", adopt mass ratio to be that the chlorine Fampridine acid of 0.1 ~ 80:0.1 ~ 80 is carried out composite with dichloro quinolinic acid.
Inventor verifies through long term test, and this above-mentioned several Herbicidal combinations mainly exists following defect:
1), by several concrete proportioning disclosed in above-mentioned several Herbicidal combinations test, find that the control of the annual broadleaf weed (as Herb of Common Nipplewort, clearvers, chickweed, common vetch etc.) to Rapeseed Field cannot play good control efficiency.
2), for several formulations disclosed in above-mentioned several Herbicidal combinations, find through verification experimental verification the defect that all there is different problem.Such as, wetting powder easily causes product to bond, not easily dispersion suspension in water, or blocking shower nozzle, the phenomenon such as reason precipitation in sprayer, cause spray irregular.
3), composite problem, by several concrete proportioning disclosed in above-mentioned several Herbicidal combinations carry out virulence test, heat storage stability test and mixture co-toxicity coefficient measure find, all cannot reach obvious synergistic effect.
Summary of the invention
An object of the present invention be to provide a kind of picloram and clopyralid compound aqueous, this aqua is reasonable in design, good to the control efficiency of the annual broadleaf weed of Rapeseed Field, and can realize the notable synergistic effect of picloram and clopyralid.
For achieving the above object, present invention employs following technical scheme:
A kind of picloram and clopyralid compound aqueous, be made up of following component according to weight portion:
Picloram is mainly used to prevent and kill off the uncultivated area block such as forest, wasteland and prevents and kill off broad-leaved assorted (annual and perennial), shrub, and domestic at present have factory to reduce be used for Controlling Weeds in Rape Fields field and wheatland broad leaved weed composite with other products.Mechanism of action suppresses mitochondria system respiration, metabolism of nucleic acid.And make chloroplast structure and other organelle developmental deformities, interferencing protein synthesizes, act on meristematic tissue activity etc., finally cause Plant death.
Clopyralid: the auxin being a kind of Prof. Du Yucang, its chemical constitution and many natural auxins similar, but in the tissue of plant, there is better persistence.It carries out absorbing then conducting in plant corpus, so its conductive performance is stronger mainly through the root of plant and leaf.After weeds dispenser, it is by the blade of plant or root absorption, moves up and down and be transmitted to rapidly whole plant in plant corpus.The clopyralid of low concentration can DNA, RNA of stimulating plant and the synthesis of protein thus cause fissional out of control and random growth, finally causes tube bank destroyed; The clopyralid of high concentration then can the division of T suppression cell and growth.Clopyralid is mainly used in rape at present, beet, flax, wheat, seeding corn and other crops prevent and kill off the broad leaved weeds such as field thistle, corn sow thistle, Herb of Common Nipplewort, common vetch.Domestic rising in 2003 starts to promote the use of this product in rape region, mainly concentrating on the rapeseed cultivation regions such as the Zhaosu County of Xinjiang Yili of China, Qinghai, Inner Mongol, Gansu, Anhui, Hubei, Sichuan, is solve Rapeseed Field field thistle, corn sow thistle, Herb of Common Nipplewort, common vetch and the unique special effect agent of Carolina Cranesbill Herb.
Picloram of the present invention and clopyralid compound aqueous, its beneficial effect shows:
1) aqua that, prepared by the present invention is all obviously better than the product prepared by other proportionings in suspensibility, persistent foamability, wet screening test etc. and heat storage stability etc.
2), verify by experiment, picloram and clopyralid with 1:4 proportioning mixed composite 30% time picloram and clopyralid compound aqueous, notable synergistic sphere of action can be played, and the preparation that other proportioning is mixed, all cannot reach notable synergistic sphere of action.Meanwhile, the actual toxicity of different ratio does not promote along with the enhancing of theoretical toxicity, there is no regular change between actual toxicity and theoretical toxicity.
Another object of the present invention is to provide a kind of picloram and the compound aqueous preparation method of clopyralid, just grind after raw material suction preparation still mix and blend through colloid mill, again through sand mill fine grinding, sample analysis, qualified rear filtration, metering, packaging, warehouse-in.
Picloram of the present invention and the compound aqueous preparation method of clopyralid, preparation technology is comparatively easy, is easy to suitability for industrialized production.
Embodiment
Below with reference to embodiment, the present invention is described in detail.But; embodiment content is only citing made for the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the design of invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
One, picloram and the compound aqueous preparation of clopyralid, and testing result, the heat storage stability result of the test of all technical of aqua prepared by each embodiment.
Embodiment 1
30% picloram and clopyralid compound aqueous, each component and weight proportion as follows:
| Composition | Weight portion |
| Picloram | 6 |
| Clopyralid | 24 |
| Fatty alcohol-polyoxyethylene ether | 3 |
| Styrylphenol polyoxyethylene ether | 5 |
| Deionized water | 62 |
Preparation method: just grind after raw material suction preparation still mix and blend through colloid mill, then through sand mill fine grinding, sample analysis, qualified rear filtration, metering, packaging, warehouse-in.
Embodiment 2
29% picloram and clopyralid compound aqueous, each component and weight proportion as follows:
| Composition | Weight portion |
| Picloram | 6 |
| Clopyralid | 23 |
| Fatty alcohol-polyoxyethylene ether | 3.5 |
| Styrylphenol polyoxyethylene ether | 4.5 |
| Deionized water | 63 |
Preparation method is with embodiment 1.
Embodiment 3
31% picloram and clopyralid compound aqueous, each component and weight proportion as follows:
| Composition | Weight portion |
| Picloram | 6 |
| Clopyralid | 25 |
| Fatty alcohol-polyoxyethylene ether | 4 |
| Styrylphenol polyoxyethylene ether | 4.5 |
| Deionized water | 60.5 |
Preparation method is with embodiment 1.
Embodiment 4
28% picloram and clopyralid compound aqueous, each component and weight proportion as follows:
| Composition | Weight portion |
| Picloram | 4 |
| Clopyralid | 24 |
| Fatty alcohol-polyoxyethylene ether | 4.5 |
| Styrylphenol polyoxyethylene ether | 4.5 |
| Deionized water | 63 |
Preparation method is with embodiment 1.
Embodiment 5
32% picloram and clopyralid compound aqueous, each component and weight proportion as follows:
| Composition | Weight portion |
| Picloram | 8 |
| Clopyralid | 24 |
| Fatty alcohol-polyoxyethylene ether | 5 |
| Styrylphenol polyoxyethylene ether | 3 |
| Deionized water | 60 |
Preparation method is with embodiment 1.
Picloram prepared by embodiment 1 ~ 5 and clopyralid compound aqueous, the testing result of product all technical is as shown in table 1, and product heat storage stability result of the test is as shown in table 2.
The testing result of a table 15 embodiment preparing product all technical
A table 25 embodiment preparing product heat storage stability result of the test
Can be found out by table 1 and 2, product prepared by embodiment 1 is all obviously better than the product prepared by other embodiments in suspensibility, persistent foamability, wet screening test etc. and heat storage stability etc.
Two, toxicological information
Picloram: rat acute per os LD
50for 2680mg/kg, acute through skin LD
50>2000mg/kg, Acute inhalation LC50 (4 hours) >5.2mg/L, non-stimulated to skin, non-stimulated to eyes.
Clopyralid: rat acute per os LD
50>5000mg/kg, acute through skin LD
50>2000mg/kg.Preparation rat acute per os LD
50female 5840mg/kg, male 4300mg/kg, acute through skin LD
50>2000mg/kg.Non-stimulated to skin, there is minimal irritation to eyes.
Three, picloram and the composite synergy indoor measurement of clopyralid
1 test objective
Under greenhouse experiment, adopt pot-culture method, the herbicidal effect of research picloram, clopyralid binary built, and the synergy type after using with both co-toxicity coefficient method evaluations different proportion of Sun Yunpei, for the rational mixture of picloram and clopyralid provides scientific basis.
2 experimental conditions
2.1 for studying thing: rape variety----Anhui oil 16
2.2 for examination weeds: Herb of Common Nipplewort, common vetch (upper one year gathered seed in field, and germination rate is more than 85%).
The cultivation of 2.3 experimental conditions and examination material
The cultivation of test material is carried out, temperature about 15 DEG C (± 2 DEG C) in illumination cultivation room.Choosing diameter is 15cm, and be highly the vinyon basin alms bowl of 15cm, the permeable hole of 1cm diameter is beaten in the bottom of basin alms bowl.Permeable hole double-layer filter paper covers, and the loam that in alms bowl, loading prepares to sterilize in advance, to alms bowl height 10cm place, soaks into soil with clear water from bottom.During test, often kind of weed seed 30-40 grain is evenly put into basin, earthing 0.5cm, the required moisture of growth between weeds culture period, should be supplemented.
2.4 other conditions
With the regular moisturizing of mode (not watering in 2 days after medicine) of bottom infiltration, keep soil moisture.
3 experimental scheme
3.1 medicament
3.1.1 reagent agent
The former medicine of 95% picloram, the former medicine of 95% clopyralid, provide by former medicine portion of Anhui Meilan Agricultural Development Co., Ltd..
3.1.2 reagent agent drug solution preparing
The medicament acetone solution prepared by embodiment 1-5, is finally diluted to desired concn with the POLYSORBATE 80 aqueous solution of 0.1% by above-mentioned former medicine.
3.2 application method
In rape 3 leaf phase, weeds 2-5 leaf phase cauline leaf spraying process dispenser 1 time.Spray medicine adopts the indoor crown-block type atomizing tester of adjustable speed, simulation field conventional spraying methods.Shower nozzle is Fan spray head, and model is Teejer8002E type, spray value 40 kgs/acre.Spray height 0.5 meter, spraying swath 0.7 meter, leg speed 0.224 meter per second.Atomisation pressure 2.0 MPa, flow 697 liters/min.
4 investigation methods
Record the damage symptoms of rape and weeds after dispenser in detail, 20d after medicine, carries out fresh weight measurement, and compared with control treatment, calculates fresh weight preventive effect.
4.1 synergy assay methods
The co-toxicity coefficient method evaluation of result of the test Sun Yunpei use with after synergy type.
Its actual toxicity index, mixture theoretical toxicity index, co-toxicity coefficient is calculated according to SUN, Y-P (Sun Yunpei) method.Take log concentration as X, damage by disease and insect preventive effect probit value is Y, asks regression equation.
Actual toxicity index=standard agent LD
50the LD of/mixture
50× 100
Theoretical toxicity index=∑ (percentage of this medicament active ingredient of the toxicity index of reagent agent × in mixture)
Actual toxicity index/theoretical toxicity index × 100 of co-toxicity coefficient=mixture
Be standard agent with clopyralid in test.
Criterion: co-toxicity coefficient <80 is antagonism, be summation action between 80-120, >120 is synergistic effect.
5 results and analysis
The co-toxicity of aqua to Herb of Common Nipplewort, common vetch prepared by embodiment 1 shows as notable synergistic effect (co-toxicity coefficient reaches 180), and aqua prepared by embodiment 2-5 only shows as addition (co-toxicity coefficient is followed successively by 85,82,83,87) to the co-toxicity of Herb of Common Nipplewort, common vetch.
Claims (2)
1. a picloram and clopyralid compound aqueous, it is characterized in that: this aqua is made up of following component according to weight portion:
2. prepare the compound aqueous method of picloram and clopyralid as claimed in claim 1 for one kind, it is characterized in that: just grind after raw material suction preparation still mix and blend through colloid mill, again through sand mill fine grinding, sample analysis, qualified rear filtration, metering, packaging, warehouse-in.
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| CN201510623912.9A CN105230626A (en) | 2015-09-25 | 2015-09-25 | Aminopyralid and clopyralid compounding aqueous agent and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103636606A (en) * | 2013-11-22 | 2014-03-19 | 重庆双丰化工有限公司 | Weed killer for preventing and removing rape field broadleaf weeds |
| WO2014092929A1 (en) * | 2012-12-14 | 2014-06-19 | Dow Agrosciences Llc | Synergistic weed control from applications of aminopyralid and clopyralid |
| CN103960243A (en) * | 2014-04-18 | 2014-08-06 | 北京明德立达农业科技有限公司 | Herbicide composition and usage thereof |
| CN104621117A (en) * | 2013-11-15 | 2015-05-20 | 南京华洲药业有限公司 | Mixed herbicide containing aminopyralid and clopyralid |
-
2015
- 2015-09-25 CN CN201510623912.9A patent/CN105230626A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014092929A1 (en) * | 2012-12-14 | 2014-06-19 | Dow Agrosciences Llc | Synergistic weed control from applications of aminopyralid and clopyralid |
| CN104621117A (en) * | 2013-11-15 | 2015-05-20 | 南京华洲药业有限公司 | Mixed herbicide containing aminopyralid and clopyralid |
| CN103636606A (en) * | 2013-11-22 | 2014-03-19 | 重庆双丰化工有限公司 | Weed killer for preventing and removing rape field broadleaf weeds |
| CN103960243A (en) * | 2014-04-18 | 2014-08-06 | 北京明德立达农业科技有限公司 | Herbicide composition and usage thereof |
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Application publication date: 20160113 |
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